CN111115620B - Preparation method of graphene quantum dots - Google Patents
Preparation method of graphene quantum dots Download PDFInfo
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- CN111115620B CN111115620B CN202010045959.2A CN202010045959A CN111115620B CN 111115620 B CN111115620 B CN 111115620B CN 202010045959 A CN202010045959 A CN 202010045959A CN 111115620 B CN111115620 B CN 111115620B
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Abstract
The invention discloses a preparation method of graphene quantum dots. One specific embodiment of the preparation method comprises the following steps: preheating the precursor to obtain a prepolymer; and dissolving the prepolymer in a solvent, and carrying out thermal synthesis reaction to obtain the graphene quantum dot. According to the embodiment of the invention, the graphene quantum dots are prepared by the two-step method, so that the preparation process is simple, and the prepared graphene quantum dots are high in yield, good in stability and high in fluorescence intensity, thereby realizing the mass production of the graphene quantum dots.
Description
Technical Field
The invention relates to the technical field of material chemistry, in particular to a preparation method of graphene quantum dots.
Background
The graphene quantum dot is a quasi-zero-dimensional nano material, and because the movement of electrons in the graphene quantum dot in all directions is limited, the quantum confinement effect of the graphene quantum dot is very obvious, and the unique physicochemical property of the graphene quantum dot brings revolutionary changes to the application of the graphene quantum in the fields of electronics, photoelectricity and electromagnetism. Compared with the traditional fluorescent material, the graphene quantum dot has the outstanding advantages of extremely high biocompatibility, fluorescence stability, controllable emission wavelength, wide excitation wavelength range, low biotoxicity, good solubility and the like, so that the graphene quantum dot becomes a good biological imaging probe, and therefore, the graphene quantum dot can be widely applied to the aspects of biosensing, biological imaging, biological drug delivery and the like.
At present, graphene quantum dots mainly have two synthesis paths of 'top-down' and 'bottom-up', but the synthesis paths are high in cost, complex in process and complex in purification, most of the synthesis paths are concentrated in a laboratory range, the yield is small, and the method is not suitable for large-scale batch industrial production. Therefore, a method which is simple in process and capable of preparing the graphene quantum dots on a large scale is provided, and is imperative for promoting the practical application and research progress of the graphene quantum dots.
Disclosure of Invention
In view of this, the embodiment of the invention provides a preparation method of graphene quantum dots, which can obtain the graphene quantum dots with high yield, good stability and high fluorescence intensity, and can realize batch production.
In order to achieve the above object, a first aspect of embodiments of the present invention provides a method for preparing graphene quantum dots. The preparation method comprises the following steps: preheating the precursor to obtain a prepolymer; and dissolving the prepolymer in a solvent, and carrying out thermal synthesis reaction to obtain the graphene quantum dot.
Further, the preheating treatment of the precursor is carried out to obtain a prepolymer, and the method comprises the following steps: and (4) preheating the precursor through a muffle furnace or an oven to obtain the prepolymer.
Further, the temperature of the pre-heating treatment is 180-200 ℃, and the time of the pre-heating treatment is 3-5 h.
Further, dissolving the prepolymer in a solvent, and performing a thermal synthesis reaction to obtain a reaction product, comprising: uniformly mixing the prepolymer and a solvent to obtain a mixed solution; placing the mixed solution in a closed reaction kettle; introducing a muffle furnace or an oven to carry out thermal synthesis reaction on the closed reaction kettle containing the mixed solution to obtain a reaction product; and carrying out post-treatment on the reaction product to obtain the graphene quantum dots.
Further, the temperature of the thermal synthesis reaction is 150-180 ℃, and the time of the thermal synthesis reaction is 40-72 h.
Further, the post-processing of the reaction product to obtain the graphene quantum dot comprises: filtering the reaction product through a filter membrane to obtain a filtrate; wherein the aperture of the filter membrane is 0.22-0.45 μm; and drying the filtrate to obtain the graphene quantum dots.
Further, the drying process includes, but is not limited to, freeze drying.
Further, the precursor is hexamethylphosphoric triamide.
Further, the solvent is one or more of ethanol, water, acetic acid, acetone, and N, N-dimethylformamide.
Further, the filling degree of the closed reaction kettle is 50-75%.
Further, the concentration of the prepolymer in the mixed solution is 0.067-0.2 g/mL.
Further, the heating rates of the preheating treatment and the thermal synthesis reaction are both 5-8 ℃/min.
Further, the filter membrane is an organic microporous filter membrane or an aqueous membrane.
Compared with the prior art, the embodiment of the invention at least has the following beneficial effects:
according to the embodiment of the invention, the graphene quantum dots are prepared by the two-step method, so that the preparation process is simple, and the prepared graphene quantum dots are good in stability, high in fluorescence intensity and high in yield, so that the mass production of the graphene quantum dots can be realized.
Drawings
Fig. 1 is a flowchart of a method for preparing graphene quantum dots in example 1 of the present invention;
fig. 2 is a fluorescence emission diagram of an aqueous solution of graphene quantum dots in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In a first aspect, an embodiment of the present invention provides a method for preparing graphene quantum dots, including the following steps: preheating the precursor to obtain a prepolymer; and dissolving the prepolymer in a solvent, and carrying out thermal synthesis reaction to obtain the graphene quantum dot.
The embodiment of the invention carries out preheating treatment on the precursor so that the precursor is partially polymerized by adsorbing and desorbing small molecules to obtain the prepolymer. That is, during the preheating treatment, a part of functional groups or small molecules in the precursor are desorbed and then undergo a polymerization reaction to obtain a prepolymer. Because the prepolymer is a relatively purified and easily-reacted raw material, the prepolymer does not need dialysis and other time-consuming and labor-consuming purification processes after thermal synthesis reaction, thereby providing guarantee for large-scale preparation of the graphene quantum dots.
The graphene quantum dot prepared by the preparation method disclosed by the embodiment of the invention has the characteristics of good thermal stability and light stability, high fluorescence intensity, strong photobleaching resistance, low toxicity and controllable emission wavelength, and is expected to replace an inorganic quantum dot to be applied to the fields of biological analysis, biological imaging and the like. In addition, compared with the traditional preparation method, the preparation method provided by the embodiment of the invention is simple in process, and can obtain the graphene quantum dots with high yield and excellent performance, so that the guarantee is provided for the large-scale production of the graphene quantum dots.
In a further embodiment, the pre-heating process on the precursor, resulting in a prepolymer, comprises: and (4) preheating the precursor through a muffle furnace or an oven to obtain the prepolymer.
Specifically, the precursor is put into a quartz boat; and (3) putting the quartz boat containing the precursor into a muffle furnace or an oven for preheating treatment to obtain the prepolymer. The embodiment of the invention carries out preheating treatment by a muffle furnace or an oven, thereby avoiding the influence of air or water vapor on the precursor polymerization reaction.
In further embodiments, the temperature of the pre-heat treatment is 180 ℃ to 200 ℃ (e.g., 180, 185, 190, 195, or 200 ℃, etc.), and the time of the pre-heat treatment is 3 to 5 hours (e.g., 3, 3.5, 4, 4.5, or 5 hours, etc.). Too high a temperature or too long a time for the preheating treatment may cause carbonization of the precursor. Therefore, by selecting proper temperature and time, part of functional groups and small molecules in the precursor can be effectively adsorbed and desorbed, so that the precursor prepolymerization reaction is facilitated.
In a further embodiment, the pre-polymer is dissolved in a solvent and subjected to a thermal synthesis reaction to yield a reaction product comprising: uniformly mixing the prepolymer and a solvent to obtain a mixed solution; placing the mixed solution in a closed reaction kettle; carrying out thermal synthesis reaction on the closed reaction kettle containing the mixed solution through a muffle furnace or an oven to obtain a reaction product; and carrying out post-treatment on the reaction product to obtain the graphene quantum dots.
Specifically, the prepolymer and the solvent are mixed by means of mechanical stirring or ultrasound, so that the prepolymer and the solvent can be fully dissolved; the mixed solution is placed in the closed reaction kettle and then heated through the muffle furnace or the oven to realize the thermal synthesis reaction, so that the influence of air or water vapor on the thermal synthesis reaction can be avoided, and the safety of the thermal synthesis reaction is improved.
According to the embodiment of the invention, the prepolymer is further subjected to graphitization, aromatization or carbonization reaction under the solvothermal condition to obtain the graphene quantum dots, so that the yield of the graphene quantum dots is improved.
It should be understood that, in order to avoid the reaction of the inner lining of the closed reaction vessel with the mixed solution and the reaction product under high temperature conditions, it is preferable that the inner lining of the closed reaction vessel is made of polytetrafluoroethylene material or polyethylene material.
In further embodiments, the thermal synthesis reaction is at a temperature of 150-. Therefore, by selecting proper temperature and time of the thermal synthesis reaction, the thermal synthesis reaction can be fully reacted, and the yield of the graphene quantum is improved.
In a further embodiment, the post-processing the reaction product to obtain the graphene quantum dot includes: filtering the reaction product through a filter membrane to obtain a filtrate; wherein the pore size of the filter membrane is 0.22-0.45 μm (e.g., 0.22, 0.3, 0.4, or 0.45 μm); and drying the filtrate to obtain the graphene quantum dots. Therefore, impurities in the graphene quantum dots can be removed through post-treatment, and the high-purity graphene quantum dots are obtained.
Specifically, the reaction product at least comprises a solvent and an unreacted precursor besides the graphene quantum dots. The reaction product is filtered to obtain a filtrate, and the graphene quantum dots are stored in the filtrate. The drying process includes, but is not limited to, freeze drying.
The graphene quantum dots prepared by the embodiment of the invention can be solution or solid powder.
In a further embodiment, the precursor is hexamethylphosphoric triamide.
In further embodiments, the solvent is one or more of ethanol, water, acetic acid, acetone, and N, N-dimethylformamide.
Further, the filling degree of the closed reaction kettle is 50-75%.
Further, the concentration of the prepolymer in the mixed solution is 0.067 to 0.2g/mL (e.g., 0.067, 0.1, 0.15, or 0.2 g/mL).
In further embodiments, the pre-heating process and the thermal synthesis reaction are each carried out at a temperature ramp rate of 4-8 deg.C/min (e.g., 4, 5, 6, 7, or 8 deg.C/min, etc.).
In further embodiments, the filter membrane is an organic-based microporous filter membrane or an aqueous-based membrane.
It is further noted that any range recited herein includes the endpoints and any values therebetween and any subranges subsumed therein or any values therebetween unless otherwise specified.
Example 1
Fig. 1 is a flowchart of a method for preparing graphene quantum dots in example 1 of the present invention; a preparation method of graphene quantum dots comprises the following steps:
s101: preheating hexamethylphosphoric triamide to obtain a prepolymer;
s102: and dissolving the prepolymer in ethanol, and carrying out thermal synthesis reaction to obtain the graphene quantum dot.
In the present embodiment, the reaction conditions and the reaction equipment of the preheating treatment and the thermal synthesis reaction are not limited as long as the graphene quantum dots of the present embodiment can be obtained.
According to the embodiment of the invention, the graphene quantum dots are prepared by the two-step method, so that the preparation process is simple, and the prepared graphene quantum dots are good in stability, high in fluorescence intensity and high in yield, so that the mass production of the graphene quantum dots can be realized.
Example 2
A preparation method of graphene quantum dots comprises the following steps:
s201: putting 5g of hexamethylphosphoric triamide into a quartz boat, then putting the quartz boat into a muffle furnace, heating the muffle furnace to 200 ℃ at the speed of 7 ℃/min, and then preheating for 3h to obtain a prepolymer;
s202: uniformly mixing 1g of prepolymer and 10mL of ethanol through mechanical stirring to obtain a mixed solution; placing the mixed solution into a closed reaction kettle with the capacity of 20mL and the inner lining of polytetrafluoroethylene; placing the closed reaction kettle in a muffle furnace, heating the muffle furnace to 160 ℃ at the speed of 5 ℃/min, and carrying out thermal synthesis reaction for 48 hours to obtain a reaction product;
s203: filtering the reaction product by an organic microporous filter membrane with the aperture of 0.45 mu m to obtain a filtrate; and (4) carrying out freeze drying treatment on the filtrate to obtain graphene quantum dot powder.
FIG. 2 is a fluorescence emission spectrum of graphene quantum dots in example 2 of the present invention; as can be seen from fig. 2, when the excitation wavelength is 339nm, the optimal emission wavelength of the graphene quantum dot is 442 nm.
And (3) irradiating the aqueous solution of the graphene quantum dots by using a UV lamp with the wavelength of 365nm, wherein the aqueous solution of the graphene quantum dots emits blue fluorescence.
The yield of the graphene quantum dots provided by the embodiment of the invention reaches 85-90%, the graphene quantum dots can still keep stable at 80 ℃, and can still keep stable after being irradiated by ultraviolet light for 1-3 days, so that the graphene quantum dots have good thermal stability and light stability.
Example 3
A preparation method of graphene quantum dots comprises the following steps:
s301: putting 10g of hexamethylphosphoric triamide into a quartz boat, then putting the quartz boat into a muffle furnace, heating the muffle furnace to 180 ℃ at the speed of 6 ℃/min, and then preheating for 5h to obtain a prepolymer;
s302: uniformly mixing 2g of prepolymer and 15mL of acetic acid through mechanical stirring to obtain a mixed solution; placing the mixed solution into a closed reaction kettle with the capacity of 20mL and the inner lining of polytetrafluoroethylene; placing the closed reaction kettle in a muffle furnace, heating the muffle furnace to 200 ℃ at the speed of 7 ℃/min, and carrying out thermal synthesis reaction for 40h to obtain a reaction product;
s303: filtering the reaction product by an organic microporous filter membrane with the aperture of 0.22 mu m to obtain a filtrate; and (4) carrying out freeze drying treatment on the filtrate to obtain graphene quantum dot powder.
In the description herein, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. A preparation method of graphene quantum dots is characterized by comprising the following steps:
preheating a precursor to obtain a prepolymer, wherein the precursor is hexamethylphosphoric triamide, the preheating temperature is 180-200 ℃, and the preheating time is 3-5 h;
uniformly mixing the prepolymer and a solvent to obtain a mixed solution;
placing the mixed solution in a closed reaction kettle;
carrying out thermal synthesis reaction on the closed reaction kettle containing the mixed solution through a muffle furnace or an oven to obtain a reaction product; the prepolymer does not need a dialysis purification process after the thermal synthesis reaction;
filtering the reaction product through a filter membrane to obtain a filtrate; wherein the aperture of the filter membrane is 0.22-0.45 μm;
and drying the filtrate to obtain the graphene quantum dots.
2. The method according to claim 1, wherein the pre-heating treatment of the precursor to obtain the prepolymer comprises: and (4) preheating the precursor through a muffle furnace or an oven to obtain the prepolymer.
3. The method as claimed in claim 1, wherein the temperature of the thermal synthesis reaction is 150 ℃ to 180 ℃, and the time of the thermal synthesis reaction is 40 to 72 hours.
4. The method of claim 1, wherein the drying process includes, but is not limited to, freeze-drying.
5. The method according to claim 1, wherein the solvent is one or more of ethanol, water, acetic acid, acetone, and N, N-dimethylformamide.
6. The method according to claim 1, wherein the concentration of the prepolymer in the mixed solution is 0.067 to 0.2 g/mL.
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